CN110615446B - Method for one-step synthesis of single-layer MWW molecular sieve by aid of amphiphilic organosilane - Google Patents
Method for one-step synthesis of single-layer MWW molecular sieve by aid of amphiphilic organosilane Download PDFInfo
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Abstract
The invention discloses a method for one-step synthesis of a single-layer MWW molecular sieve by assistance of amphiphilic organosilane, which is characterized in that a silicon dioxide sol is used as a silicon source, sodium metaaluminate is used as an aluminum source, hexamethyleneimine and dimethyloctadecyl [3- (trimethoxysilyl) propyl ] ammonium chloride are used as structure directing agents, and the single-layer MWW molecular sieve is synthesized by a one-step hydrothermal method. The synthesis method is simple and easy to implement, the yield of the synthesized product is high, and the thickness of the synthesized MWW molecular sieve nanosheet can be effectively controlled by changing the composition of the gel and the hydrothermal condition, so that the method has important significance for effectively controlling the morphology of the MWW molecular sieve and the catalytic performance of the MWW molecular sieve.
Description
Technical Field
The invention belongs to the technical field of molecular sieves and porous materials, and particularly relates to a method for one-step hydrothermal synthesis of a single-layer MWW molecular sieve by using an amphiphilic long-chain organosilane surfactant.
Background
In 1990, mobile corporation synthesized a layered molecular sieve MCM-22 with MWW topology. In 1994, leonowicz et al studied the framework structure of MCM-22 and showed that the topology was connected horizontally by MWW elementary cages to form a single sheet with shared oxygen atoms. In the vertical direction, the monolithic layers are connected by the ten-membered ring channels in the layers to form MWW sheets with a layer thickness of about 2.5 nm. MCM-22 (P) is a precursor of MCM-22, is a two-dimensional layered molecular sieve and is formed by MWW sheets in the vertical direction through hydrogen bonding force among the Si-OH sheets.
The structure determines the nature, and since MCM-22 (P) layers are bonded by hydrogen bonds, the force is weak, so that the post-treatment process can be carried out. Roasting MCM-22 (P), and dehydrating and condensing Si-OH between layers to form Si-O-Si bonds to increase dimension to form MCM-22; the composite material can also be subjected to interlayer swelling by using a surfactant, and further subjected to ultrasonic stripping to obtain the single-layer ITQ-2 molecular sieve. The ITQ-2 molecular sieve has an in-layer sinusoidal channel system which is the same as that of MCM-22, ten-membered ring sinusoidal channels connected with the supercage do not exist, mesopores generated in the stripping process enable the supercage structure to disappear, and twelve-membered ring cavities on the surfaces of the supercages are exposed on the surface of an MWW single layer, namely acid sites are exposed on the outer surface of the molecular sieve. Therefore, compared with the MCM-22 molecular sieve, the ITQ-2 molecular sieve has the advantages of large specific surface area, small micropore proportion and easy accessibility of acid sites, and can be applied to catalytic reaction of large molecules.
According to the previous literature report, the ITQ-2 molecular sieve can be obtained by performing swelling treatment on a precursor MCM-22 (P) by using an organic surfactant and then further performing ultrasonic stripping, but the process is complicated, and the swelling system (pH = 13.5-13.8, T =80 ℃) can destroy the framework structure of the molecular sieve. In view of the defects, a structure directing agent is sought, and the one-step synthesis of the single-layer MWW molecular sieve by a hydrothermal method is a hot problem in recent research.
Gemini type double-headed quaternary ammonium salt surfactant C prepared by professor of Ryoo (Nature, 2009,461,246) through elaborate design 22 H 45 -N + (CH 3 ) 2 -C 6 H 12 -N + (CH 3 ) 2 -C 6 H 13 One step in a hydrothermal system for a structure directing agentThe nano-sheet layered ZSM-5 molecular sieve is synthesized, the thickness of a laminated plate is 2nm, and the nano-sheet layered ZSM-5 molecular sieve has excellent anti-carbon deposition performance and stability in the reaction of preparing gasoline from methanol. According to the same idea, by designing a novel structure directing agent, professor Corma (angew. Chem. Int.ed.,2015,54,13724) and Luo et al (chem. Sci.,2015,6,6320) respectively successfully prepare the nano thin layer molecular sieve with MWW structure. The research results provide an important theoretical basis for the synthesis of the nano thin-layer molecular sieve. However, the structure directing agent used in the method has a complex structure and high synthesis cost, and industrial production is difficult to realize, so that the practical application of the structure directing agent is limited.
Disclosure of Invention
The invention aims to provide a method for synthesizing a single-layer MWW molecular sieve by one step through a hydrothermal method by taking an industrialized amphiphilic long-chain organosilane surfactant dimethyl octadecyl [3- (trimethoxysilyl) propyl ] ammonium chloride (TPOAC) as an auxiliary structure directing agent.
Aiming at the purposes, the technical scheme adopted by the invention comprises the following steps:
1. according to the molar ratio: siO 2 2 /Al 2 O 3 ＝30～100、OH - /SiO 2 ＝0.14～0.3、Na + /SiO 2 ＝0.14～0.3、HMI/SiO 2 ＝0.3～0.7、H 2 O/SiO 2 = 40-45, HMI/TPOAC = 2.5-6.5, wherein HMI represents hexamethyleneimine and TPOAC represents dimethyloctadecyl [3- (trimethoxysilyl) propyl group]Ammonium chloride, weighing sodium hydroxide, sodium metaaluminate, silica sol, hexamethyleneimine and dimethyl octadecyl [3- (trimethoxysilyl) propyl group]Ammonium chloride and deionized water.
2. Dissolving sodium hydroxide in deionized water completely, adding sodium metaaluminate under stirring, adding silica sol under stirring after sodium metaaluminate is dissolved completely, stirring at room temperature for 10-30 min, adding hexamethyleneimine and dimethyloctadecyl [3- (trimethoxysilyl) propyl ] ammonium chloride, and stirring at room temperature for 1-2 hr.
3. Transferring the mixed solution obtained in the step (2) into a high-pressure hydrothermal kettle with a polytetrafluoroethylene lining, and stirring and crystallizing at 140-160 ℃ under a closed condition; and after the reaction is finished, taking out the hydrothermal kettle, placing the hydrothermal kettle in cold water for quenching, washing and filtering the reaction solution, stopping washing when the filtrate is neutral, and drying the filter cake at the temperature of 60-120 ℃.
4. And (3) grinding the solid product dried in the step (3) into powder, and then placing the powder in a muffle furnace to be roasted at the temperature of 400-600 ℃ for 4-8 hours to obtain the single-layer MWW molecular sieve.
In the step 1, the molar ratio is preferably as follows: siO 2 2 /Al 2 O 3 ＝30～50、OH - /SiO 2 ＝0.2～0.3、Na + /SiO 2 ＝0.2～0.3、HMI/SiO 2 ＝0.3～0.5、H 2 O/SiO 2 Weighing raw materials of = 40-45 and HMI/TPOAC = 2.5-3.5.
In the step 3, the mixed solution obtained in the step 2 is transferred to a polytetrafluoroethylene-lined high-pressure hydrothermal kettle, and is preferably stirred and crystallized for 8 to 14 days at 150 ℃ under a closed condition.
In the above step 4, the solid product dried in the step 3 is ground into powder and then placed in a muffle furnace, preferably, for 6 hours at 500 to 550 ℃.
The invention has the following beneficial effects:
the single-layer MWW molecular sieve is hydrothermally synthesized in one step by taking silica sol as a silicon source, sodium metaaluminate as an aluminum source and Hexamethyleneimine (HMI) and dimethyloctadecyl [3- (trimethoxysilyl) propyl ] ammonium chloride (TPOAC) as structure directing agents. The preparation method is simple and easy to implement, the yield of the synthesized product is high, and the thickness of the synthesized MWW molecular sieve nanosheet can be effectively controlled by changing the composition of the gel and the hydrothermal condition, so that the method has important significance for effectively controlling the morphology of the MWW molecular sieve and the catalytic performance of the MWW molecular sieve.
Drawings
Figure 1 is an XRD pattern of MCM-22 molecular sieve and the monolayer MWW molecular sieve prepared in example 1.
FIG. 2 is an SEM image of MCM-22 molecular sieve (left) and monolayer MWW molecular sieve prepared in example 1 (right).
FIG. 3 is a TEM image of MCM-22 molecular sieve (left) and monolayer MWW molecular sieve prepared in example 1 (right).
Detailed Description
The present invention will be described in further detail with reference to the drawings and examples, but the scope of the present invention is not limited to these examples.
Example 1
1. According to the molar ratio: siO 2 2 /Al 2 O 3 ＝30、OH - /SiO 2 ＝0.2、Na + /SiO 2 ＝0.2、HMI/SiO 2 ＝0.35、H 2 O/SiO 2 =45, HMI/TPOAC =3.5, 0.13g of sodium hydroxide, 0.26g of sodium metaaluminate, 4.67g of silica sol, 1.09g of HMI, 1.56g of TPOAC, 25.16g of deionized water were weighed.
2. Completely dissolving 0.13g of sodium hydroxide in 25.16g of deionized water, then adding 0.26g of sodium metaaluminate under a stirring state, dropwise adding 4.67g of silica sol under a stirring state after the sodium metaaluminate is completely dissolved, and stirring for 30min at room temperature; then 1.09g HMI and 1.56g TPOAC were added and stirring continued at room temperature for 2h.
3. Transferring the mixed solution obtained in the step 2 into a 50mL high-pressure hydrothermal kettle with a polytetrafluoroethylene lining, and stirring and crystallizing at 150 ℃ for 60r/min for 14 days under a closed condition; and after the reaction is finished, taking out the hydrothermal kettle, placing the hydrothermal kettle in cold water for quenching, washing and filtering the reaction solution, stopping washing when the filtrate is neutral, and drying the filter cake for 12 hours at the temperature of 120 ℃.
4. And (3) grinding the solid product dried in the step (3) into powder, and then placing the powder into a muffle furnace to be roasted at 550 ℃ for 6 hours to obtain the single-layer MWW molecular sieve with the yield of 95%.
As can be seen from fig. 1, the MCM-22 molecular sieve has a distinct (002) diffraction peak and two fully split peaks between 2 θ =8 ° and 10 ° (101) and (102), indicating that the MWW layers are stacked in order to form a three-dimensional structure; compared with the MCM-22 molecular sieve, the XRD pattern of the product obtained in the embodiment has no (002) diffraction peak, and the (101) diffraction peak and the (102) diffraction peak between 2 theta = 8-10 degrees are combined into a wider peak, which indicates that the MWW type sheet layers are in a disordered arrangement state, namely the product is a single-layer MWW molecular sieve. As can be seen from FIG. 2, the single-layer MWW molecular sieve prepared in this example is arranged in a "house of cards" arrangement, unlike the MCM-22 molecular sieve. As can be seen in fig. 3, the molecular sieve prepared in this example is a single layer MWW in the (001) direction.
Example 2
1. According to the molar ratio: siO 2 2 /Al 2 O 3 ＝50、OH - /SiO 2 ＝0.2、Na + /SiO 2 ＝0.2、HMI/SiO 2 ＝0.35、H 2 O/SiO 2 =45, HMI/TPOAC =3.5, 0.18g sodium hydroxide, 0.15g sodium metaaluminate, 4.67g silica sol, 1.09g HMI, 1.56g TPOAC, 25.16g deionized water were weighed.
2. Completely dissolving 0.18g of sodium hydroxide in 25.16g of deionized water, then adding 0.15g of sodium metaaluminate under a stirring state, dropwise adding 4.67g of silica sol under a stirring state after the sodium metaaluminate is completely dissolved, and stirring for 30min at room temperature; then 1.09g HMI and 1.56g TPOAC were added and stirring continued at room temperature for 2h.
3. Transferring the mixed solution obtained in the step (2) into a high-pressure hydrothermal kettle with a 50mL polytetrafluoroethylene lining, and stirring and crystallizing for 8 days at 150 ℃ at 60r/min under a closed condition; and after the reaction is finished, taking out the hydrothermal kettle, placing the hydrothermal kettle in cold water for quenching, washing and filtering the reaction solution, stopping washing when the filtrate is neutral, and drying the filter cake for 12 hours at the temperature of 120 ℃.
4. And (4) grinding the solid product dried in the step (3) into powder, and then placing the powder in a muffle furnace to be roasted for 6 hours at 550 ℃ to obtain the single-layer MWW molecular sieve, wherein the yield is 94.1%.
Example 3
1. According to the molar ratio: siO 2 2 /Al 2 O 3 ＝30、OH - /SiO 2 ＝0.2、Na + /SiO 2 ＝0.2、HMI/SiO 2 ＝0.35、H 2 O/SiO 2 =45, HMI/TPOAC =6.5, 0.13g sodium hydroxide, 0.26g sodium metaaluminate, 4.67g silica sol, 1.09g HMI, 0.84g TPOAC, 25.16g deionized water were weighed.
2. Completely dissolving 0.13g of sodium hydroxide in 25.16g of deionized water, then adding 0.26g of sodium metaaluminate under a stirring state, dropwise adding 4.67g of silica sol under a stirring state after the sodium metaaluminate is completely dissolved, and stirring for 15min at room temperature; then 1.09g HMI and 0.84g TPOAC were added and stirring continued at room temperature for 2h.
3. Transferring the mixed solution obtained in the step 2 into a 50mL high-pressure hydrothermal kettle with a polytetrafluoroethylene lining, and stirring and crystallizing at 150 ℃ for 60r/min for 10 days under a closed condition; and after the reaction is finished, taking out the hydrothermal kettle, placing the hydrothermal kettle in cold water for quenching, washing and filtering the reaction solution, stopping washing when the filtrate is neutral, and drying the filter cake for 12 hours at the temperature of 120 ℃.
4. And (3) grinding the solid product dried in the step (3) into powder, and then placing the powder into a muffle furnace to be roasted at 550 ℃ for 6 hours to obtain the single-layer MWW molecular sieve, wherein the yield is 93.7%.
Example 4
1. According to the molar ratio: siO 2 2 /Al 2 O 3 ＝50、OH - /SiO 2 ＝0.18、Na + /SiO 2 ＝0.18、HMI/SiO 2 ＝0.3、H 2 O/SiO 2 =45, HMI/TPOAC =6.5, 0.15g sodium hydroxide, 0.15g sodium metaaluminate, 4.67g silica sol, 0.85g HMI, 1.56g TPOAC, 25.16g deionized water were weighed.
2. Completely dissolving 0.15g of sodium hydroxide in 25.16g of deionized water, then adding 0.15g of sodium metaaluminate under a stirring state, dropwise adding 4.67g of silica sol under a stirring state after the sodium metaaluminate is completely dissolved, and stirring for 30min at room temperature; then 0.85g HMI and 1.56g TPOAC were added and stirring continued at room temperature for 2h.
3. Transferring the mixed solution obtained in the step 2 into a 50mL high-pressure hydrothermal kettle with a polytetrafluoroethylene lining, and stirring and crystallizing at 150 ℃ for 60r/min for 12 days under a closed condition; and after the reaction is finished, taking out the hydrothermal kettle, placing the hydrothermal kettle in cold water for quenching, washing and filtering the reaction solution, stopping washing when the filtrate is neutral, and drying the filter cake for 12 hours at the temperature of 120 ℃.
4. And (3) grinding the solid product dried in the step (3) into powder, and then placing the powder into a muffle furnace to be roasted at 550 ℃ for 6 hours to obtain the single-layer MWW molecular sieve, wherein the yield is 94.3%.
Example 5
1、According to the molar ratio: siO 2 2 /Al 2 O 3 ＝30、OH - /SiO 2 ＝0.18、Na + /SiO 2 ＝0.18、HMI/SiO 2 ＝0.3、H 2 O/SiO 2 =40, HMI/TPOAC =3.5, 0.10g sodium hydroxide, 0.26g sodium metaaluminate, 4.67g silica sol, 1.09g HMI, 1.56g TPOAC, 22.39g deionized water were weighed.
2. Completely dissolving 0.10g of sodium hydroxide in 22.39g of deionized water, then adding 0.26g of sodium metaaluminate under the stirring state, dropwise adding 4.67g of silica sol under the stirring state after the sodium metaaluminate is completely dissolved, and stirring for 30min at room temperature; then 1.09g HMI and 1.56g TPOAC were added and stirring continued at room temperature for 2h.
3. Transferring the mixed solution obtained in the step (2) into a high-pressure hydrothermal kettle with a 50mL polytetrafluoroethylene lining, and stirring and crystallizing for 12 days at 150 ℃ at 60r/min under a closed condition; and after the reaction is finished, taking out the hydrothermal kettle, placing the hydrothermal kettle in cold water for quenching, washing and filtering the reaction solution, stopping washing when the filtrate is neutral, and drying the filter cake for 12 hours at the temperature of 120 ℃.
4. And (3) grinding the solid product dried in the step (3) into powder, and then placing the powder into a muffle furnace to be roasted at 550 ℃ for 6 hours to obtain the single-layer MWW molecular sieve, wherein the yield is 94.6%.
Example 6
In step 4 of the above examples 1 to 5, the solid product dried in step 3 was ground into powder and then calcined in a muffle furnace at 450 ℃ for 8 hours, and the other steps were the same as in example 1 to obtain a single-layer MWW molecular sieve.
Comparative example 1
In step 3 of example 1, the mixed solution obtained in step 2 was transferred to a 50mL polytetrafluoroethylene-lined high-pressure hydrothermal reactor, and crystallized under a closed condition at 150 ℃ and 60r/min with stirring for 16 days, and the other steps were the same as those of example 1, to obtain a double-layer MWW molecular sieve with a yield of 95.2%.
Comparative example 2
In step 1 of example 1, the molar ratio is: siO 2 2 /Al 2 O 3 ＝30、OH - /SiO 2 ＝0.3、Na + /SiO 2 ＝0.3、HMI/SiO 2 ＝0.5、H 2 O/SiO 2 =45, HMI/TPOAC =5, 0.25g sodium hydroxide, 0.26g sodium metaaluminate, 4.67g silica sol, 1.54g HMI, 1.56g TPOAC, 25.16g deionized water were weighed. In step 3 of example 1, the mixed solution obtained in step 2 was transferred to a 50mL polytetrafluoroethylene-lined high-pressure hydrothermal reactor, and crystallized under a closed condition at 150 ℃ and 60r/min with stirring for 7 days, and the other steps were the same as those of example 1, whereby a multilayer MWW molecular sieve was obtained with a yield of 94.8%.
Claims (1)
1. A method for one-step synthesis of a single-layer MWW molecular sieve by assistance of amphiphilic organosilane is characterized by comprising the following steps:
(1) According to the molar ratio: siO 2 2 /Al 2 O 3 =30、OH - /SiO 2 =0.2、Na + /SiO 2 =0.2、HMI/SiO 2 =0.35、H 2 O/SiO 2 =45, HMI/TPOAC =3.5, where HMI stands for hexamethyleneimine and TPOAC stands for dimethyloctadecyl [3- (trimethoxysilyl) propyl group]Ammonium chloride, weighing sodium hydroxide, sodium metaaluminate, silica sol, hexamethyleneimine and dimethyl octadecyl [3- (trimethoxysilyl) propyl ] as raw materials]Ammonium chloride and deionized water;
(2) Completely dissolving sodium hydroxide in deionized water, adding sodium metaaluminate under the stirring state, dropwise adding silicon dioxide sol under the stirring state after the sodium metaaluminate is completely dissolved, stirring at room temperature for 10-30 minutes, then adding hexamethyleneimine and dimethyloctadecyl [3- (trimethoxysilyl) propyl ] ammonium chloride, and continuously stirring at room temperature for 1-2 hours;
(3) Transferring the mixed solution obtained in the step (2) into a high-pressure hydrothermal kettle with a polytetrafluoroethylene lining, and stirring and crystallizing for 8-14 days at 150 ℃ under a closed condition; after the reaction is finished, taking out the hydrothermal kettle, placing the hydrothermal kettle in cold water for quenching, washing and filtering the reaction solution, stopping washing when the filtrate is neutral, and drying the filter cake at the temperature of 60-120 ℃;
(4) And (4) grinding the solid product dried in the step (3) into powder, and then placing the powder in a muffle furnace to be roasted for 6 hours at the temperature of 500-550 ℃ to obtain the single-layer MWW molecular sieve.
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